Water → HCID 71743833、化合物
反応式
[CH3:1][O:2][C:3]1[N:8]=[C:7]2[C:9]([CH3:23])([CH3:22])[N:10](CC3C=CC(OC)=CC=3)[C:11](=[O:12])[C:6]2=[CH:5][CH:4]=1.O.CCOC(C)=O>CC#N>[CH3:1][O:2][C:3]1[N:8]=[C:7]2[C:9]([CH3:23])([CH3:22])[NH:10][C:11](=[O:12])[C:6]2=[CH:5][CH:4]=1参加物
5
実験手順
To solution of 2-methoxy-6-(4-methoxy-benzyl)-7,7-dimethyl-6,7-dihydro-pyrrolo[3,4-b]pyridin-5-one (0.31 g, 1.0 mmol) in CH3CN (5 mL) was added ceric ammonium nitrate (1.64 g, 3.0 mmol) at room temperature. The reaction mixture was stirred at room temperature for 3 hours before water and EtOAc were added into the mixture. The organic layer was separated, dried over anhy. Na2SO4, filtered and concentrated in vacuo to give a crude product which was then purified by silica gel column chromatography to give the title compound (0.12 g, 63%) as a solid. MS: 193.1 (M+H+).
後処理
- additionwere added into the mixture
- customThe organic layer was separated
- customdried over anhy
- filtrationNa2SO4, filtered
- concentrationconcentrated in vacuo
- customto give a crude product which
- customwas then purified by silica gel column chromatography
出典と根拠
- ORDレコード
- ord-e653c4d458244b84a32a20c9b5fe75f4
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09133158B2
反応ノート
読み込み中…